CN100334269C - 一种通过电吹制纺丝法制备纳米纤维的方法及制造装置 - Google Patents

一种通过电吹制纺丝法制备纳米纤维的方法及制造装置 Download PDF

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CN100334269C
CN100334269C CNB028106695A CN02810669A CN100334269C CN 100334269 C CN100334269 C CN 100334269C CN B028106695 A CNB028106695 A CN B028106695A CN 02810669 A CN02810669 A CN 02810669A CN 100334269 C CN100334269 C CN 100334269C
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金容珉
安敬烈
成永彬
张来相
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Abstract

本发明涉及一种通过电吹制纺丝的纳米纤维网制备装置和方法。所述纳米纤维网制备方法包括：将溶解在给定溶剂中的聚合物溶液供应给纺丝喷嘴；通过加有高电压的所述纺丝喷嘴排出所述聚合物溶液，同时通过在所述纺丝喷嘴的下端附近的空气喷嘴注入压缩空气以形成纤维；以及以纤维网的形式在所述纺丝喷嘴下方的接地的抽气集合器上收集纺出的纤维。在所述方法中，热塑树脂和热固树脂都可使用，无需加热，并且很容易实现电绝缘。

Description

一种通过电吹制纺丝法制备纳米纤维的方法及制造装置
技术领域
本发明涉及一种通过电吹制纺丝(electro-blown spinning)的纳米纤维网制备装置和方法，特别涉及一种其中热塑和热固树脂都可应用、溶液不需加热并且很容易实现绝缘的纳米纤维网制备装置和方法。这里，“电吹制”是指在纳米纤维的纺丝中注入压缩空气同时施加高电压。“电吹制纺丝”则是指采用电吹制方法的纺丝。
背景技术
一般来说，由于无纺布的应用多种多样，无纺布的消费是逐步增加的，这也使得各种无纺布制造方法得到了发展。
包括美国在内的许多国家已经进行了各种研究来开发用于制造由超高精细纳米纤维(以下将称为纳米纤维网)构成的无纺布的技术。起高精细纳米纤维(ultra-fine nanofiber)比传统的超精细纤维先进了一个阶段。这类技术仍然处于初始阶段，没有进行商业化。而传统的技术则停留在这样一个阶段，即其制备出来的超精细纤维的直径约为几微米。直径约为几纳米到几百纳米的纳米纤维不能通过传统的超精细纤维技术制出。纳米纤维每单位体积的表面积之大是传统超精细纤维所无法比的。可以制出具有不同表面特征、结构和化合成分的纳米纤维，以克服由传统超精细纤维制成的物品的物理属性的限制，同时可以制出具有新性能的物品。
众所周知，采用上述纳米纤维制备方法的纳米纤维网可以被用作超高精细过滤网、电气-电子工业材料、医药生物材料以及高性能合成物等。
到目前为止，用于制备超高精细纤维的技术可以分为三种方法，包括瞬时纺丝法(flash spinning)、静电纺丝法和熔化吹制(melt-blown)纺丝法。这些技术被受让人先前提交的名称为“超高精细单纤维制备方法”的韩国专利申请第10-2001-31586号和10-2001-31587号公所开。
同时，韩国专利申请第10-2001-31586号公开了可以通过***地综合熔化吹制纺丝法和静电纺丝以高效地大规模生产和制造出纳米级的纳米纤维。图3示意性地示出了用于解释这种技术的方法。参照图3，热塑性聚合物通过漏斗10被供应给压出机12，在压出机12中热塑性聚合物被熔化成液体聚合物。熔化的液体聚合物被注入到喷丝头(spinnerette)14中，并随后与热空气一起通过纺丝喷嘴(spinningnozzle)16进入电场被纺丝。电场产生在加有电压的纺丝喷嘴16与集合器(collector)18之间。在集合器18上纺丝出的纳米纤维被抽气送风机20以网的形式收集。
韩国专利申请第10-2001-31587号还公开了可以通过***地综合熔化吹制纺丝法和静电纺丝法而高效地大规模生产和制造的纳米级的纳米纤维。图4示意性地示出了用于解释这种技术的方法。参照图4，聚合物溶液从储存槽22被注入到带有压缩泵24的喷丝头26中，并通过解压口28和随后的纺线喷嘴30进入电场被纺丝。电场产生在加以电压的纺丝喷嘴30和集合器32之间。在集合器32上纺丝出的纳米纤维被抽气送风机34以网的形式收集。
可以明白，由纳米纤维组成的纳米纤维网可根据上述两种技术制出。
然而，由于电绝缘不易形成，可以应用的树脂受到限制，并且需要加热，因此前述的传统技术有许多缺点。
发明内容
本发明就是针对解决上述问题而做出的。因此本发明的目的是提供一种纳米纤维网制备方法，在该方法中，热塑树脂和热固树脂都可使用，聚合物溶液不需被加热，并且电绝缘很容易实现。
本发明另一个目的是提供用来实现上述制备方法的纳米纤维网制备装置。
根据本发明的一个方面，为实现上述目的，本发明提供了一种纳米纤维网制备方法，包括以下步骤：将溶解在给定溶剂中的聚合物溶液供应给纺丝喷嘴；通过加有高电压的所述纺丝喷嘴排出所述聚合物溶液，同时通过在所述纺丝喷嘴的下端附近的空气喷嘴注入压缩空气以形成纤维；以及在所述纺丝喷嘴下方接地的抽气集合器上以纤维网的形式收集所述纤维。
根据本发明的另一方面，为实现上述目的，本发明提供了一种纳米纤维网制备装置，所述装置包括：储存槽，用于制备聚合物溶液；纺丝喷嘴，用于排出从所述储存槽供应的聚合物溶液；空气喷嘴，其置于所述纺丝喷嘴的下端附近，用于注入压缩空气；用于向所述纺丝喷嘴施加高电压的装置；以及接地的集合器，用于以网的形式收集从所述纺丝喷嘴排出的纺丝纤维。
附图的简要说明
图1示出了本发明所述纳米纤维网制备装置的结构；
图2A是在刀口处带有空气喷嘴的喷丝头的剖面图；
图2B是带有圆筒形空气喷嘴的另一种喷丝头的剖面图；
图3示意性地示出了通过***地综合熔化吹制纺丝法和电吹制纺丝法的纳米纤维制备方法；以及
图4示意性地示出了通过***地综合瞬时纺丝法和静电纺丝法的纳米纤维制备方法。
本发明的具体实施方式
图1示出了本发明的纳米纤维网制备装置的结构，用来说明纳米纤维网的制备方法。图2A和图2B示出了喷嘴结构，用来说明纺丝喷嘴和空气喷嘴。纳米纤维网的制备方法将参照图1至图2B得到详细描述。
通过聚合物和溶剂的混合，储存槽100制备出聚合物溶液。用于本发明的聚合物不限于热塑树脂，而可以利用大多数合成树脂，包括热固树脂。可用聚合物的例子包括聚酰亚胺、尼龙、聚芳酰胺、聚苯并咪唑、聚醚酰亚胺、聚丙烯腈、PET(聚乙烯对苯二甲酸酯)、聚丙烯、聚苯胺、聚乙烯氧化物、PEN(聚萘二甲酸乙二醇酯)，PBT(聚丁烯对苯二酯)、SBR(苯乙烯丁二烯橡胶)、聚苯乙烯，PVC(聚氯乙烯)、聚乙烯醇、PVDF(聚偏氟乙烯)、聚乙烯丁烯以及其共聚物或其派生化合物。聚合物溶液通过选择与上述聚合物相应的溶剂而制备出来。尽管图1所示的装置采用压缩结构将压缩空气或氮气强制吹入储存槽100，以从储存槽100里供应聚合物溶液。但任何不会限制聚合物溶液供应的公知装置都可被采用。聚合物溶液可以与添加剂相混合，添加剂包括可与相应聚合物兼容的任何树脂、增塑剂、紫外线稳定剂、交联剂、固化剂、反应引发剂等。强然大多数聚合物的溶解不需要任何特定的温度范围，但可能需要进行加热以帮助溶解反应。
聚合物溶液从储存槽100经过喷丝头102的纺丝喷嘴104排出。喷嘴104是电绝缘的并被加以高电压。在得到空气加热器108的加热以后，压缩空气通过安置在纺丝喷嘴104侧面的空气喷嘴106注入。
现在参考图2a和图2b，其中示出了喷丝头102中的纺丝喷嘴104和空气喷嘴106的结构。图2a示出了与图1所示相同的结构，其中空气喷嘴106被安置在纺丝喷嘴104两侧的刀口(knife edge)处。在图2a所示的纺丝喷嘴104中，聚合物溶液从上部流入纺丝喷嘴104，并经过下端的毛细管被注入。由于许多上述结构的纺丝喷嘴按照给定的间距排列在一条直线上，同时许多空气喷嘴106被安置在纺丝喷嘴104两侧的刀口处并与其排列相平行，因此使用一定数量的纺丝喷嘴104可以有利地纺丝出纳米纤维。对于各部件的优选尺度来说，每个空气喷嘴106都具有气隙“a”，其适用尺寸在约0.1mm到5mm的范围内，并且优选地约为0.5到2mm。下端毛细管具有直径“d”，其适用尺寸在约为0.1mm到2.0mm的范围内，并且优选地约为0.2到0.5mm。空气喷嘴106的下端毛细管具有适用的长度与直径比L/d，其范围约为1到20，优选地约为2到10。喷嘴凸起“e”的长度与空气喷嘴106的下端和纺丝喷嘴104的下端之间的距离相对应，并起到防止纺丝喷嘴104污染的作用。喷嘴凸起“e”的长度优选地约为-5到10mm，更特别地为0到10mm。
图2b所示的纺丝喷嘴104具有与图2a所示结构基本等同的结构，只是空气喷嘴106带有环绕纺丝喷嘴104的圆筒形结构，在这种结构中，压缩空气从通过纺丝喷嘴104纺出的纳米纤维周围的空气喷嘴106均匀地注入，因而比图2a所示的结构(也就是刀口处的空气喷嘴)具有更好的方向性。在需要大量纺丝喷嘴的情况下，纺丝喷嘴104和具有上述结构的空气喷嘴106被安置在喷丝头中。但是，这种结构的制造方法比图2a所示结构的制造方法需要付出更多的努力。
现在再次参照图1，从喷丝头的纺丝喷嘴104中排出的聚合物溶液以网的形式被收集在纺丝喷嘴104下方的抽气集合器110上。集合器110是接地的，并被设计为通过空气收集管114来抽气，空气就可以通过纺丝喷嘴104与集合器110之间的高电压区并在送风机112的吸力作用下被吸入。送风机吸入的空气包含溶剂，因此优选地设计一个溶剂回收***(SRS，未示出)来回收溶剂并同时通过其重复利用空气。所述SRS可以采用公知的结构。
在上述制备方法的结构中，施加电压的部分或接地的部分明显地与其它部分分开，从而容易地实现了电绝缘。
本发明通过空气喷嘴106注入压缩空气而通过集合器110吸入空气，这样就能将喷嘴污染减到最小并且成为本发明的最佳优点。虽然上面没有清楚描述，但在通过除熔化吹制纺丝法之外的纺丝制备方法中，喷嘴污染是非常严重的阻碍因素。通过压缩空气的注入和吸入，本发明能将喷嘴污染减到最小。由于因喷嘴凸起“e”的调整而注入的压缩空气能够清洗喷嘴，所以喷嘴凸起“e”更优选的功能是清除喷嘴污染。
另外，可以在集合器上安置各种衬底用以在衬底上收集并合成纺出的纤维网，从而使这种合成纤维网可被用作高性能过滤器、手帕(wiper)等。所述衬底的例子可以包括各无纺布，如熔化吹制的无纺布、针织和纺织花边(spunlace)无纺布、纺织布、针织布、纸等，并且只要纳米纤维层能够被添加到衬底上，衬底的使用就可以不受限制。
本发明具有下述方法条件。
施加在喷丝头102上的电压优选地在约1到300kV范围内，更优选地约为10到100kV。聚合物溶液可在0.01到1.96×107Pa(200kg/cm2)的压力范围下排出，优选地在0.1到1.96×106Pa(20kg/cm2)的压力范围下排出。这样使得聚合物溶液能够大量排出，从而满足大量制造纳米纤维的需要。与静电纺丝方法相比，本发明的方法能够以大约0.1到5cc/分钟-孔的高排放率排出聚合物溶液。
通过空气喷嘴106注入的压缩空气具有约10到10000米/分钟的流速，优选地约为100到3000米/分钟。空气温度优选地为室温到约300℃的范围，更优选地为室温到约100℃的范围。冲模到集合器的距离(Die to Collector Distance-DCD)，也就是纺丝喷嘴104的下端与抽气集合器110之间的距离，优选地约为1到200cm，更优选地为10到50cm。
下面将在随后的例子是更详细地描述本发明。
利用聚丙烯腈(PAN)作为聚合物并以DMF作为溶剂，制备出具有20W％浓度的聚合物溶液，并随后用如图1所示的具有刀口处空气喷嘴的喷丝头进行纺丝。聚合物溶液根据下列条件被纺丝：纺丝喷嘴的直径约为0.25mm，喷嘴的L/d为10，DCD为200mm，纺丝压力为5.88×105Pa(6kg/cm2)，并且所施加的电压为直流50kV。
具有如图1所示结构的刀口处的喷丝头在以下例子中得到使用。纺丝喷嘴的直径为0.25mm，喷嘴的L/d为10，DCD在例1到例3中是变化的，并在例4到例10中被设为300mm。纺丝喷嘴的数量为500，冲模(Die)的宽度为750mm，喷嘴凸起“e”约为0到3mm，通过空气喷嘴的压缩空气的流速保持在300到3000米/分钟。
表1
序号   聚合物   溶剂   浓度(％)    DCD(mm)     纺丝压力[105Pa(kgf/cm2)]   施加的电压(kV)
例1   PAN   DMF   15    350     3   30
例2   PAN   DMF   20    160     4   40
例3   PAN   DMF   20    200     6   50
对比例1   PAN   DMF   25
例1的流动性和纺丝能力良好，但网的构造较差。例2和例3的流动性、纺丝能力和网的构造良好。对SEM图片的检测表明纤维直径分布在500nm到2μm之间。具体而言，在例3中可以看出。纤维直径分布在500nm到1.2μm范围内。在对比例1中，很难制备出25％的PAN溶液，所以不能获得任何成效。
表2
    序号     纺丝压力[105Pa(kgf/cm2)]     施加的电压(kV)     直径分布(nm)
    例4     3     21     933.96-1470
    例5     3     30     588.69-1000
    例6     2.9     40     500.9-970.8
    例7     3     60     397.97-520.85
    例8     3.1     80     280.01-831.60
    例9     3.5     40     588.69-933.77
    例10     4     40     633.9-1510
表2报告了例4到例10的条件和结果，其中使用尼龙66作为聚合物，使用蚁酸作为溶剂，聚合物溶液的浓度为25％的纤维。表2中的纤维直径分布是SEM(扫描电子显微镜)图片检测的结果，其中纳米纤维以网状形式不规则地排列。
工业应用
如上面所阐明的，本发明形成网，所述网由纤维直径范围从几纳米到几百纳米的纳米纤维组成。另外，本发明的制备方法比传统的静电纺丝方法具有更高的排放率，因而有大量制造纳米纤维的潜力。另外，由于使用了聚合物溶液，本发明具有加热聚合物的需求被减少、热塑和热固树脂都能使用的优点。
此外，在用于电吹制纺丝的结构中，喷丝头能够很容易地实现电绝缘，同时溶剂能够通过抽取而被回收。

Claims (16)

1.一种纳米纤维网制备方法，包括以下步骤：
将溶解在给定溶剂中的聚合物溶液供应给纺丝喷嘴；
通过加有高电压的所述纺丝喷嘴排出所述聚合物溶液，同时通过与所述纺丝喷嘴的下端附近的空气喷嘴注入压缩空气以形成纤维；以及
在所述纺丝喷嘴下方接地的抽气集合器上以纤维网的形式收集所述纤维。
2.根据权利要求1所述的纳米纤维网制备方法，其特征在于，加到所述纺丝喷嘴的电压为1到300kV。
3.根据权利要求1所述的纳米纤维网制备方法，其特征在于，所述聚合物溶液在压力范围为0.01到1.96×107Pa的排放压力下通过所述纺丝喷嘴被压缩排出。
4.根据权利要求1所述的纳米纤维网制备方法，其特征在于，所述压缩空气的流速为10到10000米/分钟。并且其温度为室温到300℃。
5.根据权利要求4所述的纳米纤维网制备方法，其特征在于，所述压缩空气的温度为室温到100℃。
6.根据权利要求1所述的纳米纤维网制备方法，其特征在于，所述纤维网直接在所述集合器上被纺丝。
7.根据权利要求1所述的纳米纤维网制备方法，其特征在于，所述纤维网被纺丝到所述集合器上设置的衬底上。
8.根据权利要求1所述的纳米纤维网制备方法，其特征在于，所述聚合物是从以下群组中选出的一种，所述群组包括：聚酰亚胺、尼龙、聚芳酰胺、聚苯并咪唑、聚醚酰亚胺、聚丙烯腈、PET(聚乙烯对苯二甲酸酯)、聚丙烯、聚苯胺、聚乙烯氧化物、PEN(聚萘二甲酸乙二醇酯)，PBT(聚丁烯对苯二酯)、SBR(苯乙烯丁二烯橡胶)、聚苯乙烯，PVC(聚氯乙烯)、聚乙烯醇、PVDF(聚偏氟乙烯)、聚乙烯丁烯以及其共聚物或其派生化合物。
9.一种用于制备纳米纤维网的纳米纤维网制备装置，包括：
储存槽，用于制备聚合物溶液；
纺丝喷嘴，用于排出从所述储存槽供应的聚合物溶液；
空气喷嘴，其置于所述纺丝喷嘴的下端附近，用于注入压缩空气；
用于向所述纺丝喷嘴施加高电压的装置；以及
接地的集合器，用于以网的形式收集从所述纺丝喷嘴排出的纺丝纤维。
10.根据权利要求9所述的纳米纤维网制备装置，进一步包括设于所述纺丝喷嘴的下部内的毛细管，其特征在于，所述毛细管的直径为0.1到2mm，其长度与直径之经为1到20。
11.根据权利要求9所述的纳米纤维网制备装置，其特征在于，所述用来注入压缩空气的空气喷嘴被安置在所述纺丝喷嘴两侧的刀口处，并且具有0.1到5.0mm的间隔或气隙。
12.根据权利要求9所述的纳米纤维网制备装置，其特征在于，所述空气喷具有环绕所述纺丝喷嘴的圆筒形，并具有0.1到5.0mm的宽度或气隙。
13.根据权利要求9所述的纳米纤维网制备装置，其特征在于，所述纺丝喷嘴的下端与所述集合器的间隔为1到200cm。
14.根据权利要求9所述的纳米纤维网制备装置，进一步包括用于将空气从纺丝空间抽到所述集合器中的送风机，其特征在于，所述送风机将空气供应到用于回收溶剂的溶剂回收***。
15.根据权利要求9所述的纳米纤维网制备装置，其特征在于，一喷嘴凸起对应于空气喷嘴的下端与纺丝喷嘴的下端之间的高度差，所述喷嘴凸起为0mm到10mm。
16.根据权利要求9所述的纳米纤维网制备装置，其特征在于进一步包括用于将所述聚合物溶液从所述储存槽供应给所述纺丝喷嘴的泵。
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